CN107573074B - Method for preparing laminated SiC-based impact-resistant composite ceramic material at low temperature by RMI method - Google Patents
Method for preparing laminated SiC-based impact-resistant composite ceramic material at low temperature by RMI method Download PDFInfo
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Abstract
The invention relates to a method for preparing a laminated SiC-based impact-resistant composite ceramic material at low temperature by an RMI method, wherein a ceramic film is prepared by a tape casting method, the ceramic film obtained after drying and demoulding is cut, and laminated alternately to obtain a laminated ceramic preform; preparing a ceramic biscuit by carrying out dry pressing, low-temperature hot pressing and cold isostatic pressing on the laminated ceramic preform; and performing high-temperature heat treatment to ensure that the laminated SiC-based impact-resistant ceramic has corresponding strength, and performing RMI to prepare the laminated SiC-based impact-resistant ceramic. Compared with the prior art, the laminated SiC-based impact-resistant composite ceramic material prepared by the RMI method at low temperature has the effects of macroscopic and microscopic lamination toughening and reinforcement, and realizes the multi-scale effect; meanwhile, the casting method is combined with the low-temperature hot pressing process, so that the porosity can be effectively reduced, the defects can be reduced, the interlayer bonding force can be enhanced, the strength of the ceramic biscuit can be improved, and the method has good popularization and application values.
Description
Technical Field
The invention belongs to the field of ceramic composite materials, relates to a method for preparing a laminated SiC-based impact-resistant composite ceramic material at a low temperature by an RMI method, in particular to a method for preparing a high-strength and high-toughness laminated SiC-based impact-resistant composite ceramic material by combining a tape casting method and an RMI method, and particularly relates to a method for preparing a laminated SiC-based impact-resistant composite ceramic material at a low temperature by an RMI method.
Background
The low toughness is one of the common defects of ceramic materials, and the layered ceramic improves the toughness of the material while ensuring the higher strength of the ceramic materials by using the structural design of bionics to form an energy dissipation structure. The layered ceramic is formed by replacing laminated layers with two materials with different moduli, so that the modulus matching is realized, and the toughness of the material is further improved. The strong layer with higher modulus is used for bearing, and the soft layer with lower modulus is used for deflecting cracks to absorb energy. Therefore, the structural design of the layered ceramic can improve the performance of the material while ensuring certain strength, and prevent the material from catastrophic brittle fracture and from shattering when receiving high-speed impact.
At present, the preparation process of the laminated ceramic mainly comprises a prefabricated substrate and a final sintering process. The prefabricated substrate mainly comprises a tape casting method, a coating method and a dry powder laminating method; the sintering modes of the laminated ceramics of the SiC system (SiC/ZrB2, SiC/TiC, SiC/BN and SiC/C) mainly comprise hot-pressing sintering, spark plasma sintering and the like. Wherein the hot-pressing sintering needs to be prepared at a certain pressure above 1900 ℃; the discharge plasma sintering has higher requirements on equipment, the preparation cost of the two modes is higher, and the prepared sample has limited size and is not suitable for industrial production. Therefore, a ceramic preparation process of the SiC-based laminated ceramic, which is low in cost and suitable for industrial production, is needed.
The reaction melting siliconizing method (RMI) is a common method for preparing SiC ceramics at low temperature, and has the advantages of low preparation temperature (1450-1650 ℃), low cost, simple process and suitability for industrial production. The method is widely used for preparing carbon-ceramic brake discs, impact-resistant block ceramics and the like. Patent document CN1887794A discloses a method for preparing SiC/Si or SiC/BN layered ceramic by in-situ reaction, which comprises cutting paper into certain size, soaking in phenolic resin, taking out, air drying, laminating, pressing, drying, carbonizing, siliconizing, and discharging silicon to obtain SiC-based layered composite ceramic. However, due to the limitation of raw material paper and process, the thickness of the prepared substrate is limited, the designability of the structure is poor, the variety of the prepared laminated ceramic is limited, and the prepared material has too many residual defects to cause the performance of the material, such as strength, toughness and the like, and is not suitable for industrial production.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing a laminated SiC-based impact-resistant composite ceramic material at a low temperature by an RMI method.
Technical scheme
A method for preparing a laminated SiC-based impact-resistant composite ceramic material at low temperature by an RMI method is characterized by comprising the following steps:
step 1, preparation of casting sheet: preparing a ceramic film by adopting a tape casting method, drying and demoulding; the ceramic film comprises the following components: 35-50 parts of powder, 5-15 parts of carbon, 40-55 parts of solvent, 2-5 parts of dispersant, 5-10 parts of binder and 2-5 parts of plasticizer;
the powder is SiC powder, TiC powder and B4C powder and Si3N4Powder or Si powder;
the solvent is a mixed solution of methyl ethyl ketone and ethanol, and the methyl ethyl ketone and the ethanol are mixed according to the volume ratio of 1:1-2: 1;
the binder is polyvinyl butyral;
the plasticizer is a mixed solution of glycerol and dioctyl phthalate, and the glycerol and the dioctyl phthalate are mixed according to the volume ratio of 1:2-1: 1;
cutting and alternately laminating the dried and demoulded ceramic film according to design requirements, and forming a prefabricated body by dry pressing at 5-10 MPa; then placing the mixture into a 100-plus-200 ℃ oven for heat preservation for 1-3h, and then carrying out low-temperature hot pressing under the pressure of 5-10 MPa; then carrying out cold isostatic pressing at the pressure of 150 and 200MPa for 1-5min to prepare a layered ceramic preform;
step 3, preparing ceramic biscuit:
placing the laminated ceramic preform into a tube furnace, heating to 600 ℃ at the speed of 1 ℃/min, and carrying out heat preservation for 2h to carry out glue removal; continuously heating to 1000-1300 ℃ at the speed of 1.5 ℃/min, and preserving heat for 1h to perform high-temperature heat treatment to form a ceramic biscuit;
step 4, preparing the laminated impact-resistant SiC-based composite ceramic material:
embedding the ceramic biscuit with silicon powder and placing the ceramic biscuit in a graphite crucible, placing the graphite crucible in a vacuum furnace, heating to 1500-1650 ℃ at the speed of 10-15 ℃/min, preserving heat for 1-3h, and cooling to room temperature along with the furnace to obtain the laminated SiC-based impact-resistant composite ceramic.
The preparation of the casting sheet in the step 1 is as follows: mixing and grinding the powder, carbon, solvent and dispersant to obtain a premixed solution, adding a binder and a plasticizer to mix to obtain casting slurry, carrying out vacuum defoaming on the casting slurry, and passing through a casting machine to obtain the ceramic film.
The weight parts of the raw materials in the step 1 are respectively as follows: siC powder or TiC powder or B4C powder or Si3N440-45 parts of powder or Si powder, 8-10 parts of carbon, 45-51 parts of solvent, 3-5 parts of dispersant, 8-9 parts of binder and 3-5 parts of plasticizer.
The dispersant is one or more of polyvinylpyrrolidone, triolein, triethyl phosphate and castor oil.
The grain diameter of each powder is 1-20 μm.
Advantageous effects
The invention provides a method for preparing a laminated SiC-based impact-resistant composite ceramic material at low temperature by an RMI method, which comprises the steps of preparing a ceramic film by a tape casting method, cutting the ceramic film obtained after drying and demoulding, and alternately laminating to obtain a laminated ceramic preform; preparing a ceramic biscuit by carrying out dry pressing, low-temperature hot pressing and cold isostatic pressing on the laminated ceramic preform; and performing high-temperature heat treatment to ensure that the laminated SiC-based impact-resistant ceramic has corresponding strength, and performing RMI to prepare the laminated SiC-based impact-resistant ceramic.
Compared with the prior art, the method has the following advantages:
(1) the preparation process combining the tape casting method and the RMI method effectively reduces the preparation temperature of the laminated SiC-based impact-resistant composite ceramic, increases the matching types of different layers, realizes the designability of the structure and is suitable for industrial production;
(2) the laminated SiC-based impact-resistant composite ceramic prepared by the RMI method has the effects of toughening and reinforcing macroscopic and microscopic layers, and realizes the multi-scale effect;
(3) the casting method is combined with the low-temperature hot pressing process, so that the porosity can be effectively reduced, the defects can be reduced, the interlayer bonding force can be enhanced, and the strength of a ceramic biscuit can be improved;
(4) selecting TiC powder and B4C powder and Si3N4Powder and Si powder as materials for preparing laminated ceramic, and Ti powder can be formed3SiC2Layer, B4C layer, Si3N4Layer, ZrO2The layer, the Si layer and the SiC layer are matched to prepare the high-performance laminated SiC-based impact-resistant ceramic composite material, wherein Ti is3SiC2Is itself oneThe layered material has high ductility, low hardness, high yield strength, high melting point, high heat stability and good oxidation resistance, can maintain high strength at high temperature, has a microscopic layered structure capable of playing a good role in absorbing energy when bearing high-speed impact resistance, and can enable layered ceramics to bear multiple impacts without crushing damage, and B4C and Si3N4The composite material has high hardness and high mechanical property of high melting point, and can be matched with a SiC layer in hardness to prepare the laminated impact-resistant ceramic with excellent performance and resistance to armor piercing; the Si layer has the property of metalloid, can generate certain plastic deformation, and improves the toughness of the material; the SiC layer is subjected to performance matching with the different layers to form a good energy dissipation structure, so that not only can a macroscopic designable laminated structure be realized, but also a microscopic laminated structure is realized, a multi-scale effect is realized, and the performance of the material is greatly improved;
(5) the laminated SiC-based impact-resistant composite ceramic prepared by the RMI method has excellent high-speed impact resistance and mechanical properties.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a laminated SiC-based impact-resistant composite ceramic material at a low temperature by an RMI method;
FIG. 2 is an XRD pattern of a layered SiC-based impact resistant composite ceramic prepared in example 1;
FIG. 3 is a surface scanning electron microscope image of a layered SiC-based impact-resistant composite ceramic layered structure prepared in example 1;
FIG. 4 is a back-scattered scanning electron microscope image of the laminated SiC-based impact resistant composite ceramic prepared in example 1;
FIG. 5 is a scanning electron microscope image of the cross-sectional morphology of the laminated SiC-based impact-resistant composite ceramic prepared in example 1;
FIG. 6 is a scanning electron microscope image of crack propagation of the layered SiC-based impact resistant composite ceramic prepared in example 1;
FIG. 7 is a scanning electron microscope image of the cross-sectional morphology of the laminated SiC-based impact-resistant composite ceramic prepared in example 2;
FIG. 8 is a scanning electron microscope image of the cross-sectional morphology of the laminated SiC-based impact-resistant composite ceramic prepared in example 3.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the technical task of the invention is realized in the following way, and the method comprises the following steps:
(1) and preparing a casting sheet: preparing a ceramic film by adopting a tape casting method, wherein the ceramic film is a SiC film or a TiC film or B4C film or Si3N4A thin film or a Si thin film;
(2) preparing a layered prefabricated body: cutting the ceramic film obtained after drying and demoulding, and designing different layer thickness ratios to carry out alternate lamination to obtain a laminated ceramic prefabricated body;
(3) and preparing a ceramic biscuit: preparing a ceramic biscuit by the layered ceramic preform through dry pressing, low-temperature hot pressing and cold isostatic pressing;
(4) and preparing the laminated impact-resistant SiC-based composite ceramic material: and (3) after the ceramic biscuit is subjected to high-temperature thermal treatment after glue discharging, the ceramic biscuit is made to have corresponding strength, and then RMI is carried out to prepare the laminated SiC-based impact-resistant ceramic.
Preferably, the preparation of the cast sheet in the step (1) comprises the following steps:
35-50 parts of SiC powder, TiC powder or B4C powder or Si3N4Adding powder or Si powder, 5-15 parts of carbon, 40-55 parts of solvent and 2-5 parts of dispersant into a spherical ink tank, and mixing for 24-48h to obtain a premixed solution;
secondly, adding 5-10 parts by weight of binder and 2-5 parts by weight of plasticizer into the premixed liquid, and mixing for 24-48 hours to obtain casting slurry;
and thirdly, removing bubbles of the casting slurry in vacuum, adjusting the heights of scrapers in front of and behind the casting machine, and casting, drying and demolding to obtain the ceramic film.
Preferably, the weight parts of the raw materials in the step (1) are respectively as follows: SiC powder or TiC powder or B4C powder or Si3N440-45 parts of powder or Si powder, 8-10 parts of carbon, 45-51 parts of solvent, 3-5 parts of dispersant, 8-9 parts of binder and 3-5 parts of plasticizer.
Preferably, the solvent in the step (1) is a mixed solution of methyl ethyl ketone and ethanol, and the methyl ethyl ketone and the ethanol are mixed according to a volume ratio of 1:1-2: 1.
Preferably, the dispersant in the step (1) is one or more of polyvinylpyrrolidone, triolein, triethyl phosphate and castor oil, and is preferably triethyl phosphate.
Preferably, the grain diameter of the powder in the step (1) is 1-20 μm.
Preferably, in the step (1), the adhesive is polyvinyl butyral, the plasticizer is a mixed solution of glycerol and dioctyl phthalate, and the glycerol and the dioctyl phthalate are mixed according to the volume ratio of 1:2-1: 1.
More preferably, the preparation of the layered preform in step (2) comprises the following steps:
firstly, cutting, alternately laminating and dry-pressing the ceramic film at 5-10MPa to obtain a prefabricated body with a corresponding size;
secondly, putting the dry-pressed prefabricated body into a 100-200 ℃ baking oven for heat preservation for 1-3h, quickly taking out the prefabricated body, and realizing low-temperature hot pressing under the pressure of 5-10 MPa;
and thirdly, 150-200MPa cold isostatic pressing for 1-5min to obtain the layered ceramic preform.
More preferably, the preparation of the ceramic biscuit in the step (3) comprises the following steps:
firstly, placing the laminated ceramic preform into a tube furnace, heating to 600 ℃ at the speed of 1 ℃/min, and carrying out heat preservation for 2h to remove glue;
secondly, the temperature is continuously increased to 1000-1300 ℃ at the speed of 1.5 ℃/min, and the temperature is kept for 1h for high-temperature heat treatment, so that the strength of the ceramic biscuit is enhanced, and the cracking of the biscuit body can not occur in the RMI process.
Preferably, the preparation of the layered impact-resistant SiC-based composite ceramic material in the step (4) comprises the following steps:
secondly, embedding the ceramic biscuit subjected to high-heat treatment by using silicon powder and placing the ceramic biscuit into a graphite crucible;
secondly, placing the graphite crucible in a vacuum furnace, heating to 1500-1650 ℃ at the speed of 10-15 ℃/min, preserving the heat for 1-3h, and cooling to room temperature along with the furnace to obtain the laminated SiC-based impact-resistant composite ceramic.
The specific embodiment is as follows:
example 1:
as shown in attached figures 1, 2, 3, 4, 5 and 6, the RMI method of the invention is a method for preparing a laminated SiC-based impact-resistant composite ceramic material at a low temperature, and the method comprises the following steps:
(1) the preparation method of the casting sheet comprises the following specific steps:
adding 40kg of SiC powder, 5kg of carbon, 51kg of mixed solution of methyl ethyl ketone and ethanol and 2kg of triethyl phosphate into a spherical ink tank, and mixing for 24 hours to obtain premixed liquid, wherein the methyl ethyl ketone and the ethanol are mixed according to the volume ratio of 1: 1; the particle size of the powder is 1 mu m;
adding 5kg of polyvinyl butyral and 2kg of mixed solution of glycerol and dioctyl phthalate into the premixed solution, and mixing for 24 hours to obtain casting slurry, wherein the glycerol and the dioctyl phthalate are mixed according to the volume ratio of 1: 1;
and thirdly, removing bubbles of the casting slurry in vacuum, adjusting the heights of scrapers in front of and behind the casting machine, and casting, drying and demolding to obtain the SiC ceramic film.
40kg of SiC powder is replaced by 40kg of TiC powder to obtain the TiC ceramic film.
(2) The preparation method of the layered prefabricated body comprises the following specific steps:
firstly, cutting, alternately laminating and dry-pressing a ceramic film at 10MPa to obtain a prefabricated body with a corresponding size;
secondly, putting the dry-pressed preform into a drying oven at 100 ℃ for heat preservation for 1h, quickly taking out the preform, and realizing low-temperature hot pressing under the pressure of 10 MPa;
and thirdly, cold isostatic pressing at 200MPa, and keeping the pressure for 5min to prepare the laminated ceramic preform.
(3) The preparation of the ceramic biscuit comprises the following specific steps:
firstly, placing the laminated ceramic preform into a tube furnace, heating to 600 ℃ at the speed of 1 ℃/min, and carrying out heat preservation for 2h to remove glue;
secondly, continuously heating to 1100 ℃ at the speed of 1.5 ℃/min, and preserving heat for 1h to carry out high-temperature heat treatment, so as to enhance the strength of the ceramic biscuit and ensure that the biscuit does not crack in the RMI process.
(4) The preparation method of the laminated impact-resistant SiC-based composite ceramic material comprises the following specific steps:
firstly, embedding the ceramic biscuit subjected to high-heat treatment by using silicon powder and placing the ceramic biscuit into a graphite crucible;
secondly, placing the graphite crucible into a vacuum furnace, heating to 1600 ℃ at the speed of 10 ℃/min, preserving heat for 1h, and cooling to room temperature along with the furnace to obtain the layered SiC/Ti3SiC2Impact-resistant composite ceramics.
The thickness of the thin sheet prepared by the tape casting method can be 0.05mm to 0.3mm, the thickness of each layer is controlled by controlling the number of the thin sheets, and the designability of the layer thickness ratio is further realized, so that the performance of the thin sheet can meet different application requirements. For example, the laminated SiC/TiC ceramic with the layer thickness ratio of 10:1 needs to be designed: the thickness of the SiC thin slice prepared by casting is 0.2mm, the thickness of TiC is 0.1mm, 5 SiC casting thin slices are required to be overlapped together, and then the SiC casting thin slices are overlapped with 1 TiC casting thin slice, the thickness ratio of the SiC thin slices to the TiC casting thin slices is a structural unit with the thickness ratio of 10:1, and the laminated ceramic with the designable layer thickness ratio is prepared by overlapping a plurality of structural units.
Example 2:
as shown in the attached figure 7, the RMI method of the invention is used for preparing the laminated SiC-based impact-resistant composite ceramic material at low temperature, and the method comprises the following steps:
(1) the preparation method of the casting sheet comprises the following specific steps:
adding 35kg of SiC powder, 10kg of carbon, 46kg of mixed solution of methyl ethyl ketone and ethanol and 3kg of triethyl phosphate into a spherical ink tank, and mixing for 24 hours to obtain premixed liquid, wherein the methyl ethyl ketone and the ethanol are mixed according to the volume ratio of 2: 1; the particle size of the powder is 1 mu m;
adding 8kg of polyvinyl butyral and 3kg of mixed solution of glycerol and dioctyl phthalate into the premixed solution, and mixing for 24 hours to obtain casting slurry, wherein the glycerol and the dioctyl phthalate are mixed according to the volume ratio of 1: 2;
and thirdly, removing bubbles of the casting slurry in vacuum, adjusting the heights of scrapers in front of and behind the casting machine, and casting, drying and demolding to obtain the SiC ceramic film.
At 35kgB4The C powder replaces 35kg of SiC powder to obtain B4C, a ceramic film.
(2) The preparation method of the layered prefabricated body comprises the following specific steps:
firstly, cutting, alternately laminating and dry-pressing a ceramic film at 5MPa to obtain a prefabricated body with a corresponding size;
secondly, putting the dry-pressed preform into a 200 ℃ oven for heat preservation for 3 hours, quickly taking out the preform, and realizing low-temperature hot pressing under the pressure of 5 MPa;
and thirdly, cold isostatic pressing at 150MPa, and keeping the pressure for 1min to prepare the laminated ceramic preform.
(3) The preparation of the ceramic biscuit comprises the following specific steps:
firstly, placing the laminated ceramic preform into a tube furnace, heating to 600 ℃ at the speed of 1 ℃/min, and carrying out heat preservation for 2h to remove glue;
secondly, the temperature is continuously increased to 1200 ℃ at the speed of 1.5 ℃/min, and the temperature is kept for 1h for high-temperature heat treatment, so that the strength of the ceramic biscuit is enhanced, and the cracking of the biscuit body is avoided in the RMI process.
(4) The preparation method of the laminated impact-resistant SiC-based composite ceramic material comprises the following specific steps:
firstly, embedding the ceramic biscuit subjected to high-heat treatment by using silicon powder and placing the ceramic biscuit into a graphite crucible;
secondly, placing the graphite crucible into a vacuum furnace, heating to 1650 ℃ at the speed of 15 ℃/min, preserving heat for 3h, and cooling to room temperature along with the furnace to obtain the layered SiC/B4C impact-resistant composite ceramic.
Example 3:
as shown in the attached figure 8, the RMI method of the invention is used for preparing the laminated SiC-based impact-resistant composite ceramic material at low temperature, and the method comprises the following steps:
(1) the preparation method of the casting sheet comprises the following specific steps:
adding 45kg of SiC powder, 8kg of carbon, 40kg of mixed solution of methyl ethyl ketone and ethanol and 5kg of triethyl phosphate into a spherical ink tank, and mixing for 24 hours to obtain premixed liquid, wherein the methyl ethyl ketone and the ethanol are mixed according to the volume ratio of 1: 1; the particle size of the powder is 10 mu m;
adding 5kg of polyvinyl butyral and 5kg of mixed solution of glycerol and dioctyl phthalate into the premixed solution, and mixing for 24 hours to obtain casting slurry, wherein the glycerol and the dioctyl phthalate are mixed according to the volume ratio of 1: 1;
and thirdly, removing bubbles of the casting slurry in vacuum, adjusting the heights of scrapers in front of and behind the casting machine, and casting, drying and demolding to obtain the SiC ceramic film.
At 45kgSi3N4The powder replaces 45kg of SiC powder to obtain Si3N4A ceramic membrane.
(2) The preparation method of the layered prefabricated body comprises the following specific steps:
firstly, cutting, alternately laminating and dry-pressing a ceramic film at 10MPa to obtain a prefabricated body with a corresponding size;
secondly, putting the dry-pressed preform into a drying oven at 100 ℃ for heat preservation for 1h, quickly taking out the preform, and realizing low-temperature hot pressing under the pressure of 10 MPa;
and thirdly, cold isostatic pressing at 200MPa, and keeping the pressure for 5min to prepare the laminated ceramic preform.
(3) The preparation of the ceramic biscuit comprises the following specific steps:
firstly, placing the laminated ceramic preform into a tube furnace, heating to 600 ℃ at the speed of 1 ℃/min, and carrying out heat preservation for 2h to remove glue;
secondly, continuously heating to 1300 ℃ at the speed of 1.5 ℃/min, and preserving heat for 1h for high-temperature heat treatment to enhance the strength of the ceramic biscuit so as to ensure that the biscuit does not crack in the RMI process.
(4) The preparation method of the laminated impact-resistant SiC-based composite ceramic material comprises the following specific steps:
firstly, embedding the ceramic biscuit subjected to high-heat treatment by using silicon powder and placing the ceramic biscuit into a graphite crucible;
secondly, placing the graphite crucible into a vacuum furnace, heating to 1650 ℃ at the speed of 10 ℃/min, preserving heat for 1h, and cooling to room temperature along with the furnace to obtain the laminated SiC/Si3N4Impact-resistant composite ceramics.
Example 4:
the invention discloses a method for preparing a laminated SiC-based impact-resistant composite ceramic material at low temperature by an RMI method, which comprises the following steps:
(1) the preparation method of the casting sheet comprises the following specific steps:
adding 50kg of SiC powder or 15kg of carbon, 45kg of mixed solution of methyl ethyl ketone and ethanol and 3kg of triethyl phosphate into a spherical ink tank, and mixing for 24 hours to obtain premixed liquid, wherein the methyl ethyl ketone and the ethanol are mixed according to the volume ratio of 1: 1; the particle size of the powder is 20 mu m;
adding 9kg of polyvinyl butyral and 3kg of mixed solution of glycerol and dioctyl phthalate into the premixed solution, and mixing for 24 hours to obtain casting slurry, wherein the glycerol and the dioctyl phthalate are mixed according to the volume ratio of 1: 1;
and thirdly, removing bubbles of the casting slurry in vacuum, adjusting the heights of scrapers in front of and behind the casting machine, and casting, drying and demolding to obtain the SiC ceramic film.
50kg of SiC powder was replaced with 50kg of Si powder to obtain a Si ceramic thin film.
(2) The preparation method of the layered prefabricated body comprises the following specific steps:
firstly, cutting, alternately laminating and dry-pressing a ceramic film at 10MPa to obtain a prefabricated body with a corresponding size;
secondly, putting the dry-pressed preform into a drying oven at 100 ℃ for heat preservation for 1h, quickly taking out the preform, and realizing low-temperature hot pressing under the pressure of 10 MPa;
and thirdly, cold isostatic pressing at 200MPa, and keeping the pressure for 5min to prepare the laminated ceramic preform.
(3) The preparation of the ceramic biscuit comprises the following specific steps:
firstly, placing the laminated ceramic preform into a tube furnace, heating to 600 ℃ at the speed of 1 ℃/min, and carrying out heat preservation for 2h to remove glue;
secondly, continuously heating to 1000 ℃ at the speed of 1.5 ℃/min, and preserving heat for 1h for high-temperature heat treatment to enhance the strength of the ceramic biscuit so as to ensure that the biscuit does not crack in the RMI process.
(4) The preparation method of the laminated impact-resistant SiC-based composite ceramic material comprises the following specific steps:
firstly, embedding the ceramic biscuit subjected to high-heat treatment by using silicon powder and placing the ceramic biscuit into a graphite crucible;
secondly, placing the graphite crucible in a vacuum furnace, heating to 1550 ℃ at the speed of 10 ℃/min, preserving heat for 1h, and cooling to room temperature along with the furnace to obtain the laminated SiC/Si impact-resistant composite ceramic.
And (3) testing the effect: the test results are shown in the following table:
Claims (4)
1. a method for preparing a laminated SiC-based impact-resistant composite ceramic material at low temperature by an RMI method is characterized by comprising the following steps:
step 1, preparation of casting sheet: preparing a ceramic film by adopting a tape casting method, drying and demoulding; the ceramic film comprises the following components: 40-45 parts of powder, 8-10 parts of carbon, 45-51 parts of solvent, 3-5 parts of dispersant, 8-9 parts of binder and 3-5 parts of plasticizer;
the powder is SiC powder, TiC powder and B4C powder and Si3N4Powder or Si powder;
the solvent is a mixed solution of methyl ethyl ketone and ethanol, and the methyl ethyl ketone and the ethanol are mixed according to the volume ratio of 1:1-2: 1;
the binder is polyvinyl butyral;
the plasticizer is a mixed solution of glycerol and dioctyl phthalate, and the glycerol and the dioctyl phthalate are mixed according to the volume ratio of 1:2-1: 1;
step 2, preparing a layered preform:
the ceramic film is prepared by taking the dried and demoulded powder as SiC powder, and the powder is TiC powder and B4C powder and Si3N4Cutting and alternately laminating the ceramic film prepared from the powder or the Si powder according to the design requirement, and forming a prefabricated body by dry pressing at 5-10 MPa; then placing the mixture into a 100-plus-200 ℃ oven for heat preservation for 1-3h, and then carrying out low-temperature hot pressing under the pressure of 5-10 MPa; then, 150-MPa cold isostatic pressing is carried out, the pressure maintaining time is 1-5min, and the layered ceramic prefabricated part is preparedA body;
step 3, preparing ceramic biscuit:
placing the laminated ceramic preform into a tube furnace, heating to 600 ℃ at the speed of 1 ℃/min, and carrying out heat preservation for 2h to carry out glue removal; continuously heating to 1000-1300 ℃ at the speed of 1.5 ℃/min, and preserving heat for 1h to perform high-temperature heat treatment to form a ceramic biscuit;
step 4, preparing the laminated impact-resistant SiC-based composite ceramic material:
embedding the ceramic biscuit with silicon powder and placing the ceramic biscuit in a graphite crucible, placing the graphite crucible in a vacuum furnace, heating to 1500-1650 ℃ at the speed of 10-15 ℃/min, preserving heat for 1-3h, and cooling to room temperature along with the furnace to obtain the laminated SiC-based impact-resistant composite ceramic.
2. The RMI method of claim 1 is used for preparing the laminated SiC-based impact-resistant composite ceramic material at low temperature, and is characterized in that: the preparation of the casting sheet in the step 1 is as follows: mixing and grinding the powder, carbon, solvent and dispersant to obtain a premixed solution, adding a binder and a plasticizer to mix to obtain casting slurry, carrying out vacuum defoaming on the casting slurry, and carrying out casting to obtain the ceramic film.
3. The RMI method of claim 1 or 2, which is a method for preparing a laminated SiC-based impact-resistant composite ceramic material at a low temperature, wherein: the dispersant is one or more of polyvinylpyrrolidone, triolein, triethyl phosphate and castor oil.
4. The RMI method of claim 1 or 2, which is a method for preparing a laminated SiC-based impact-resistant composite ceramic material at a low temperature, wherein: the grain diameter of each powder is 1-20 μm.
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